CN1078257A - 1,1,2,3, the azeotropic shape composition of 3-pentafluoropropane - Google Patents

1,1,2,3, the azeotropic shape composition of 3-pentafluoropropane Download PDF

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Publication number
CN1078257A
CN1078257A CN93102338A CN93102338A CN1078257A CN 1078257 A CN1078257 A CN 1078257A CN 93102338 A CN93102338 A CN 93102338A CN 93102338 A CN93102338 A CN 93102338A CN 1078257 A CN1078257 A CN 1078257A
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weight
contain
carbon atom
azeotropic
compositions
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拉吉特·塞伯拉·巴索
彼得·布莱恩·劳格斯顿
里奥那德·迈克尔·斯塔舒拉
厄尔·A·E·伦德
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Honeywell International Inc
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AlliedSignal Inc
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G5/00—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents
    • C23G5/02—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents using organic solvents
    • C23G5/028—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents using organic solvents containing halogenated hydrocarbons
    • C23G5/02803—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents using organic solvents containing halogenated hydrocarbons containing fluorine
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
    • C11D7/50—Solvents
    • C11D7/5036—Azeotropic mixtures containing halogenated solvents
    • C11D7/5068—Mixtures of halogenated and non-halogenated solvents
    • C11D7/5077—Mixtures of only oxygen-containing solvents
    • C11D7/5081—Mixtures of only oxygen-containing solvents the oxygen-containing solvents being alcohols only

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  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
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  • Oil, Petroleum & Natural Gas (AREA)
  • General Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Detergent Compositions (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Manufacturing Of Printed Wiring (AREA)
  • Fire-Extinguishing Compositions (AREA)
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Abstract

The present invention relates to contain 1,1,2,3,3-pentafluoropropane and methyl alcohol or ethanol and the some compositions that maybe can also contain Nitromethane 99Min., they are very stable, can be used as degreasing agent and solvent, be used to comprise dry-cleaning and the cold rinse of printed-wiring board (PWB) and the various industrial cleaning use of deflux.

Description

1,1,2,3, the azeotropic shape composition of 3-pentafluoropropane
Use solvent based on fluorine carbon to carry out vapor degreasing and solvent cleaning has been widely used for removing the greasy dirt of solid surface and the cleaning of others in industry, the greasy dirt that is difficult to remove especially for the parts and the cleaning of cleaning structure complexity.
The simple form of vapor degreasing or solvent cleaning method is exactly to be in the steam that object places boiling solvent cruelly that is cleaned of room temperature.Devaporation just provides clean through the distillatory solvent, for the usefulness of flush away greasy dirt and other contamination on object.Solvent final evaporation from the object is fallen, and can't resemble with the direct cleaning of liquid solvent and stay residue.
The dirt of removing for difficulty, (need improving temperature) or need carry out the fabrication line operation of the large volume of effective Rapid Cleaning for metal parts and assembly parts to promote the cleanup action of solvent, the routine operation of vapor degreasing device is exactly that the parts that will clean are immersed in earlier in the boiling solvent pond to remove the greasy dirt of main amount, then parts are immersed in again and are equipped with in the pond of new distillatory near the solvent of room temperature, at last parts are put cruelly in the solvent vapour on boiling pool, steam then condenses on the parts that are cleaned.In addition, last steam purge before this step also available through the distillatory solvent to the parts cleaning of spraying.
Cold rinse has been to use the another kind of method of some kinds of solvents, in the operation of most of cold rinse, with the greasy dirt parts or be immersed in the solvent liquid, or has the things such as rag of solvent to wipe with soaking, and makes it at air drying then.
In recent years, the fluorocarbon solvent such as Refrigerant R 113 is widely used as effective, nontoxic and nonflammable chemical reagent in degreasing cleaning and other solvent cleaning.Have found that Refrigerant R 113 has gratifying solvent to greasy dirt, oil, wax etc. and renders a service.Therefore it has been widely used in the cleaning of electric motor, compressor, heavy metal parts, exquisite Precise Alloy parts, printed-wiring board (PWB), gyrostat, guidance system, space flight and guided missile hardware, aluminium parts etc.
The composition of azeotropic or azeotropic shape is sought after, because they can fractionation in when boiling, this character is desirable just, because in the vapor degreasing equipment of aforementioned these solvents of use, the distillatory solvent liquid of having regenerated again is used for last drip washing.Therefore, the effect such as the same distiller of this vapor degreasing system.Unless solvent compositions has the constant boiling point, promptly this composition is the azeotropic shape, otherwise the fractionation phenomenon will take place, and will cause that unfavorable solvent composition distributes, thereby disturb cleaning process and security thereof.If solvent mixture is not the azeotropic shape, wherein volatile components will preferably evaporate, just produced some mixtures of different compositions, they have unfavorable character, and for example the solvability to oil reduces, metal, plastics or elastomeric unreactiveness minimizing, combustibility and toxicity are increased.This technical field contains the azeotropic or the azeotropic shape composition of needed fluorine carbon component such as Refrigerant R 113 always in expectation, the component that these compositions comprised can also produce the required character of other, polar functionality for example, bigger solvability and stability.
The technician in this field is seeking the new azeotropic shape mixture based on fluorine carbon, hydrogen fluorine carbon and hydrochlorofluorocarazeotropic always, so that provide available thing for the new and special purposes of degreasing and other cleaning.At present, they are considered to the best safe quid pro quo of hydrogen fluorine carbon (CFCs) material that uses at present to it should be noted that chloride minimum or not chloride azeotropic shape mixture based on fluorine carbon, hydrogen fluorine carbon and hydrochlorofluorocarazeotropic especially.People suspect that Chlorofluorocarbons class material can cause environmental problem aspect the earth ozone layer.Mathematical model is verified with such as 1,1,2-three chloro-1,2, the Chlorofluorocarbons class of 2-Halothane (CFC-113) is compared, resemble 1,1,2,3, the hydrogen fluorine carbon of 3-pentafluoropropane (prior art is called HFC-245ea) can not produce detrimentally affect aspect atmospheric chemistry, its effect and global greenhouse effect that consumes ozone all is negligible.
The European patent 431,458 that on June 12nd, 1991 delivered has disclosed 1,1,2,3,4,4-hexafluoro butane and alcoholic acid mixture.United States Patent (USP) 5,023,010 has disclosed 1,1,1,2,3, the azeotropic mixture of 3-hexafluoro-3-methoxy propane and methyl alcohol.United States Patent (USP) 5,035,830 have disclosed hexafluoropropylene/ethylene cyclic dimer and methyl alcohol or alcoholic acid constant boiling mixture.United States Patent (USP) 5,064,559 have disclosed 1,1,1,2,3,4,4,5,5,5-Decafluoropentane and methyl alcohol or alcoholic acid constant boiling mixture.United States Patent (USP) 5,073,291 have disclosed 1, the constant boiling mixture of 4-dihydro perfluorinated butane and methyl alcohol.
United States Patent (USP) 5,073,288 and 5,073,290 have disclosed 1,1,1,2,2,3,5,5,5-nine fluoro-4-trifluoromethyl pentane or 1,1,1,2,2,5,5,5-octafluoro-4-trifluoromethyl pentane and methyl alcohol or alcoholic acid binary azeotropic shape composition.
The measure that solves the needs that substitute the Chlorofluorocarbons solvent among the present invention is to use and contains 1,1,2,3,3-pentafluoropropane and methyl alcohol or ethanol and the mixture that maybe can also contain Nitromethane 99Min..In addition, also found to contain 1,1,2,3,3-pentafluoropropane and methyl alcohol or ethanol and maybe can also contain Nitromethane 99Min., and be that new azeotropic shape is a boiling point constant composition.
Be preferably, this new azeotropic shape composition contains 1,1,2,3 of significant quantity, 3-pentafluoropropane and methyl alcohol or ethanol and presumable Nitromethane 99Min..Here the term of usefulness " significant quantity " is meant the consumption of each component that can form this azeotropic shape composition of combining with other component.
This azeotropic shape composition contains the 89-99.99%(weight of having an appointment) 1,1,2,3,3-pentafluoropropane, about 0.01-11%(weight) methyl alcohol or ethanol and the about 1%(weight of 0-) Nitromethane 99Min..
Because underlying cause, azeotropic shape composition of the present invention is very favourable.1,1,2,3, the ozone-depleting amount that the 3-pentafluoropropane causes can be ignored, and its boiling point is 40 ℃, and methyl alcohol and ethanol component have good solvent property.Like this, when these components combine with significant quantity, just obtained effectively azeotropic shape solvent.
Following table has been listed some preferred azeotropic shape compositions, and wherein 1,1,2,3, the 3-pentafluoropropane is abbreviated as HFC-245ea.In table, digital scope is interpreted as titled with " pact " word.
Figure 931023386_IMG1
Composition in the compositing range of pointing out in table and some particular composition that exceeds this scope all are the azeotropic shapes by the specific definitions of having done below.
The definite composition of azeotropic composition is not measured as yet, but has determined it is within above-mentioned scope.No matter real azeotrope is formed and where to be positioned at, all be the azeotropic shape composition of following specific definitions at above-mentioned some particular composition of pointing out the composition of scope and exceeding this scope.
Here the term of usefulness " azeotropic shape composition " is the composition that its character of expression resembles azeotrope, promptly has constant boiling point characteristic and also promptly do not have the fractionation tendency when boiling or evaporation.Like this, in this based composition, the composition of the steam that forms when boiling or evaporation is identical or practically identical with the composition of primary liquid.Therefore, when boiling or evaporation, also only be on minimum or insignificant degree, to change if liquid is formed change.These are different with non-azeotropic shape composition, and latter's liquid when boiling or evaporation is formed the change that significance degree is arranged.As this technical elements personnel were easy to understand, the boiling point of azeotropic shape composition changes with pressure.
Azeotropic shape composition of the present invention is used as solvent in various application such as vapor degreasing, cold rinse and solvent cleaning comprise deflux and dry-clean.
In method embodiment of the present invention, the degreasing equipment that employing such as immersion or spraying or use are conventional or the like the known any method of this technical field, thus make said composition can be used to clean solid surface with azeotropic shape compositions-treated solid surface of the present invention.In a method embodiment of the present invention, by such as immersing or spraying or the conventional known any methods of this technical field such as degreasing equipment that can in fact remove or dissolve dirt of use, can or remove crude removal from this surface dissolving with the surface of azeotropic shape compositions-treated base material of the present invention.
According to for example J.Burdon etc. at " making the tetrahydrofuran (THF) partially fluorinated " J.of Chem.Soc(C with cobaltic fluoride), any currently known methods that makes commercially available tetrahydrofuran (THF) and cobaltic fluoride reaction that 1739(1969) is disclosed in the literary composition can make of the present invention 1,1,2,3, the 3-pentafluoropropane.In this new azeotropic shape composition of using as solvent of the present invention, all be known materials as for these components of methyl alcohol, ethanol and Nitromethane 99Min., can buy from the market.
Embodiment 1
In the present embodiment, the Schwellenwert that boiling point is formed curve to composition is in 95%(weight) 1,1,2,3,3-pentafluoropropane (calling HFC-245ea in the following text) and 5%(weight) in the zone of methyl alcohol, this shows an azeotrope generation near this forms.
Used a little generator, it is a 15ml round bottom double-neck flask that has magnetic stirring bar, heats with electric mantle.About 2.5ml low boiling component HFC-245ea is added generator in a subtle way earlier, by the automatic injector that can press the microlitre injection methyl alcohol is added by amount again.Measure temperature and measure barometrical pressure with platinum-resistance thermometer.The boiling point of measuring is made correction to obtain the boiling point under the 760mmHg.
To the different all mixtures of the composition of HFC-245ea and methyl alcohol measure its boiling point and revise to its at 760mmHg(101Kpa) under the boiling point value.In the data that push away show that the Schwellenwert of boiling point is in about 2.4-9%(weight) in the zone of methyl alcohol.The minimum best estimate of boiling point is in 4.7%(weight) the methyl alcohol place, though in 0.5-10%(weight) in the zone of methyl alcohol, the boiling point of each mixture all is constant within 0.4 ℃.So just show that the minimum boiling point azeotrope is present in this compositing range.
We had not planned the compositing range of boiling point constant group compound made completely and had defined.Any technician in this field can be not difficult to determine the boiling point constant or in fact constant contain other mixture of this same composition.
Embodiment 2
Except using the ethanol instead of methanol, repeat embodiment 1 in others, earlier about 2.8ml low boiling component HFC-245ea is added generator in a subtle way, add ethanol by the automatic injector that can press the microlitre injection by amount ground then.For HFC-245ea and all mixtures of alcoholic acid measure its boiling point and revise to its at 760mmHg(101Kpa) value.Push away expression in the data, minimum boiling point is positioned at about 0.1-0.8%(weight) the alcoholic acid scope.Though in 0.01-2%(weight) in the alcoholic acid compositing range, the boiling point of mixture is all constant within 0.2 ℃, the best estimate of boiling point extreme lower position is in 0.5%(weight) ethanol place.Like this, just show that the minimum boiling point azeotrope is in this compositing range.
Embodiment 3 and 4
Thereby come the clean metal test specimen to carry out its Research on effect as solvent with azeotropic shape composition of the present invention.Metal specimen oils its band with various types of oil respectively, and being heated to 93 ℃ is having machining in the presence of these oil and grinding the temperature that is reached partly to imitate.
The metal specimen of handling like this is placed on degreasing in the three pond formula vapor phase deoiling machines.In this typical three pond formula deoiling machines, the condensing worm that is looped around machine edge is used for making the solvent vapour condensation, and phlegma then is collected in earlier in the pond, then phlegma again overflow go in some compact cascade type ponds, enter boiling pool at last.
Metal specimen is placed in the solvent vapour, cleaned 15 seconds to 2 minutes, the concrete time is looked the kind of oil of band that sample coupon is stained with and different.With the azeotropic shape composition of embodiment 1 and 2 as solvent.Thereby the test specimen washing test is to make the residue that stays after the cleaning with the weight change of analytical balance measurement test button spare to carry out.
Embodiment 5 and 6
Solvent with embodiment 1 and 2 under 27 ℃ adds (with 50: 50 ratio) in the mineral oil respectively.These two kinds of solvents all respectively can be miscible with mineral oil.
Embodiment 7 and 8
Test button spare is oiled with various oil bands, and the metal specimen that will be stained with band oil was immersed in the solvent of embodiment 1 and 2 about 15 seconds to 2 minutes, took out metal specimen, made its dry air, and visual inspection shows that in fact its oil of being stained with band all removed.
Embodiment 9 and 10
With various types of oil test button spare band is oiled, be stained with the metal specimen that oils of band, make its dry air then with the cleaning of spraying of the solvent of embodiment 1 and 2.Visual inspection shows that in fact its oil of being stained with band all removed.
Also adding some known additives in azeotropic shape composition of the present invention makes composition can be applicable to specific purposes.Inhibitor can be added in the azeotropic shape composition of the present invention, its objective is the decomposition of composite inhibiting, decompose the unfavorable product that produces with composition and react, and/or prevent the corrosion of metallic surface.Arbitrary inhibitor or all inhibitor in the following kind all can be used among the present invention: the alkanol with 4-7 carbon atom, itroparaffin with 2-3 carbon atom, have 1 of 2-7 carbon atom, 2-epoxy group(ing) paraffinic hydrocarbons, has the phosphoric acid ester of 12-30 carbon atom, ethers with 3-4 carbon atom, ethers with 3-4 carbon atom, unsaturated compound with 4-6 carbon atom, acetals with 4-7 carbon atom, the amine that has the ketone of 3-5 carbon atom and have 6-8 carbon atom.Other suitable inhibitor also is not difficult to adopt concerning the technician in this field.In spray method, available thruster is sprayed on azeotropic shape composition on the test specimen surface.
Above-mentioned inhibitor can be a kind of with it, or use its mixture with any ratio.The typical amounts of inhibitor is the about 2%(weight that accounts for azeotropic shape composition).

Claims (10)

1, some permanent Azeotrope-like compositions is characterized in that containing 1,1,2,3 of the 89-99.99% (weight) that has an appointment, 3-pentafluoropropane, the Nitromethane 99Min. of the methyl alcohol of about 0.01-11% (weight) or ethanol and 0-about 1% (weight).
2, azeotropic shape compositions more according to claim 1, it is characterized in that being actually by about 89-99.5%(weight) 1,1,2,3,3-pentafluoropropane, about 0.5-11%(weight) methyl alcohol and about 0-1%(weight) Nitromethane 99Min. form, the boiling point of described these compositions is about 38.1 ℃ at 760mmHg.
3, azeotropic shape composition according to claim 1, it is characterized in that being actually by about 90-98.2%(weight) 1,1,2,3,3-pentafluoropropane, about 1.8-10%(weight) methyl alcohol and 0-0.5%(weight) Nitromethane 99Min. form, the boiling point of described these compositions is about 38.1 ℃ at 760mmHg.
4, azeotropic shape composition according to claim 1, it is characterized in that being actually by about 90.6-97.6%(weight) 1,1,2,3,3-pentafluoropropane, about 2.4-9.4%(weight) methyl alcohol and about 0-0.4%(weight) Nitromethane 99Min. form, the boiling point of described these compositions is about 38.1 ℃ at 760mmHg.
5, azeotropic shape composition according to claim 1, it is characterized in that being actually by about 97-99.99%(weight) 1,1,2,3,3-pentafluoropropane, about 0.01-3%(weight) ethanol and about 0-1%(weight) Nitromethane 99Min. form, the boiling point of described these compositions is about 38.5 ℃ under 760mmHg.
6, azeotropic shape composition according to claim 1, it is characterized in that being actually by about 98.5-99.99%(weight) 1,1,2,3,3-pentafluoropropane, about 0.01-1.5%(weight) ethanol and about 0-0.5%(weight) Nitromethane 99Min. form, the boiling point of described these compositions is about 38.5 ℃ at 760mmHg.
7, azeotropic shape composition according to claim 1, it is characterized in that being actually by about 98.8-99.99%(weight) 1,1,2,3,3-pentafluoropropane, about 0.01-1.2%(weight) ethanol and about 0-0.4%(weight) Nitromethane 99Min. form, the boiling point of described these compositions is about 38.5 ℃ under 760mmHg.
8, azeotropic shape composition according to claim 1, it is characterized in that described these compositions also contain a kind of inhibitor in addition, it optional from contain 4-7 carbon atom the alkane alcohols, contain 2-3 carbon atom the itroparaffin class, contain 1 of 2-7 carbon atom, 2-epoxy group(ing) alkanes, contain 12-30 carbon atom phosphoric acid ester, contain 3 or 4 carbon atoms ethers, contain 4-6 carbon atom unsaturated compound, contain the acetals of 4-7 carbon atom, the amine that contains the ketone of 3-5 carbon atom and contain 6-8 carbon atom.
9, azeotropic shape composition according to claim 2, it is characterized in that described these compositions also contain a kind of inhibitor in addition, it optional from contain 4-7 carbon atom the alkane alcohols, contain 2-3 carbon atom the itroparaffin class, contain 1 of 2-7 carbon atom, 2-epoxy group(ing) alkanes, contain 12-30 carbon atom phosphoric acid ester, contain 3 or 4 carbon atoms ethers, contain 4-6 carbon atom unsaturated compound, contain the acetals of 4-7 carbon atom, the amine that contains the ketone of 3-5 carbon atom and contain 6-8 carbon atom.
10, a kind ofly promptly remove the method for crude removal, it is characterized in that the step that it comprises is to adopt the described azeotropic shape of claim 2 composition as solvent from substrate surface dissolving.
CN93102338A 1992-04-27 1993-02-19 1,1,2,3, the azeotropic shape composition of 3-pentafluoropropane Pending CN1078257A (en)

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US07/873,861 US5219490A (en) 1992-04-27 1992-04-27 Azeotrope-like compositions of 1,1,2,3,3-pentafluoropropane
US873,861 1992-04-27

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US5073288A (en) * 1990-08-17 1991-12-17 E. I. Du Pont De Nemours And Company Compositions of 1,1,1,2,2,3,5,5,5-nonafluoro-4-trifluoromethylpentane and use thereof for cleaning solid surfaces
US5064559A (en) * 1990-10-11 1991-11-12 E. I. Du Pont De Nemours And Company Binary azeotropic compositions of (CF3 CHFCHFCF2 CF3) with methanol or ethanol or isopropanol

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US9382504B2 (en) 2008-12-19 2016-07-05 3M Innovative Properties Company Composition and method to provide stain release and stain repellency properties to substrates
CN102317235B (en) * 2008-12-19 2017-10-31 3M创新有限公司 The composition and method of greasiness removal and pollution resistance are provided for substrate
CN102161941A (en) * 2011-03-14 2011-08-24 耿建 Environment-friendly hydrocarbon cleaning agent
CN102161941B (en) * 2011-03-14 2012-06-20 天津市安晟瑞信清洗剂有限公司 Hydrocarbon cleaning agent
CN104862126A (en) * 2015-05-22 2015-08-26 上海中孚特种油品有限公司 Environment-friendly flame-retardant solvent cleaner and preparation method thereof
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US5219490A (en) 1993-06-15
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SG49809A1 (en) 1998-06-15
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TW228548B (en) 1994-08-21
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JPH07506141A (en) 1995-07-06
HK1007174A1 (en) 1999-04-01
EP0638131A1 (en) 1995-02-15
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DE69310170D1 (en) 1997-05-28

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